CN101654438A - Imidazole ionic liquid production technology - Google Patents
Imidazole ionic liquid production technology Download PDFInfo
- Publication number
- CN101654438A CN101654438A CN200910065927A CN200910065927A CN101654438A CN 101654438 A CN101654438 A CN 101654438A CN 200910065927 A CN200910065927 A CN 200910065927A CN 200910065927 A CN200910065927 A CN 200910065927A CN 101654438 A CN101654438 A CN 101654438A
- Authority
- CN
- China
- Prior art keywords
- ionic liquid
- production technology
- hours
- liquid
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an imidazole ionic liquid production technology, belonging to the new material field. The production technology process includes that: N-methyl imidazoie and halogenated hydrocarbon are pumped into a reaction tank in mol ratio of 1:1-1.9, stirring and heating in water bath are carried out, the temperature is controlled to be 20-95 DEG C, and reaction lasts 24-96 hours, so as to obtain halogen ionic liquid; and corresponding anion salt is added, stirring and heating in water bath are carried out, the temperature is controlled to be 20-95 DEG C, and reaction lasts 24-96 hours, so as to obtain corresponding ionic liquid. The reactant is subject to standing for layering, and washing, purifying and reduced pressure distillation are carried out to obtain products. The technological process is simple and controllable and is applicable to scale production of imidazoie ionic liquid.
Description
One. technical field:
The present invention relates to a kind of ionic liquid scale production process, particularly a kind of glyoxaline ion liquid scale production process belongs to field of new.
Two. background technology:
Ionic liquid claims the room temperature melting salt again, is a kind of in room temperature or be bordering on the ionic compound that is in a liquid state under the room temperature, does not have electroneutral molecule in ionic liquid, the 100%th, constitute by organic cation and inorganic or organic anion.Compare with the organic solvent of present widespread use, ionic liquid has: advantage such as the liquid scope of broad, extremely low vapour pressure, wide electrochemical window, favorable conductive and thermal conductivity, good light transmittance and high refractive index, high specific heat capacity and energy storage, high thermal stability, selective dissolution power and designability, reusable edible.The incomparable characteristic of other liquid that ionic liquid had, make it can be applicable to high-tech areas such as organic synthesis, extracting and separating, electrochemistry, biocatalysis, environmental improvement, functional material, the new space of transforming is provided not only for traditional chemical reaction, and for the greenization process of chemical engineering provides a brand-new field, the problem of environmental pollution that the solution modern industry is brought will have breakthrough simultaneously, be a kind of ideal green chemical solvents.
Ionic liquid at room temperature in the research is mainly the imidazoles material at present, such ionic liquid has advantages such as insensitive to empty G﹠W, that fusing point is lower, application number is 200710063267.5 be entitled as " a kind of ionic liquid and its production and use " to disclose a kind of employing supercritical co to do solvent, react under certain temperature and time, washing, purifying make the glyoxaline ion liquid of aromatic hydrocarbons or naphthenic hydrocarbon replacement; Application number is 200410018529.2 be entitled as " a kind of synthetic method of water soluble ion liquid " to disclose a kind of employing supersonic cell crusher to prepare ion liquid method; Same application number is that 02824172.X is entitled as " preparing ion liquid method " and discloses the ion liquid method of a kind of ultrasonicization of employing preparation.Yet these many research reports only limit to laboratory lab scale rank; ion liquid large-scale production is not found as yet; and if above a few class ionic liquid production technologies are amplified; can exist facility investment bigger; the shortcoming that reaction conditions is had relatively high expectations etc.; certainly will increase ion liquid production cost, be difficult to realize industrialization.
Three. summary of the invention:
The present invention provides a kind of scale production process of glyoxaline ion liquid for overcoming above all deficiencies.
A kind of imidazole ionic liquid production technology provided by the present invention, such ion liquid general structure is
In the formula:
R1 is the saturated hydrocarbyl that contains 1～20 carbon atom;
X
-For inorganic or organic ion unit, comprising: Cl
-, Br
-, BF
4 -, PF
6 -, CH
3COO
-, CF
3COO
-
Its production process is: N-Methylimidazole and halon was extracted in the retort by the mole proportioning in 1: 1～1: 1.9, stirs, and heating in water bath, temperature is controlled at 20～95 ℃, reacts 24～96 hours, can obtain the halogen ionic liquid; Further add respective anionic salt, stir, heating in water bath, temperature is controlled at 20～95 ℃, reacts 24～96 hours, can get corresponding ionic liquid.With the reactant standing demix, the washing purifying, underpressure distillation obtains product.All reactants and solvent are liquid state or solution form, adopt vacuum to take out material.Adopt methylene dichloride to make solvent for water soluble ion liquid, the methylene dichloride in the reaction process is recycled by underpressure distillation.
Imidazole ionic liquid production technology provided by the present invention, when accomplishing scale production, it is simple to have equipment, easy handling, reaction conditions is less demanding, product purity height, advantage such as energy-efficient.
Four. embodiment:
The present invention illustrates with following embodiment, but the present invention is not limited to following embodiment, under the scope of described aim, changes and implements to be included in the technical scope of the present invention before and after not breaking away from.
Embodiment 1
1-butyl-3-Methylimidazole villaumite
50kgN-Methylimidazole and 80kg n-propylcarbinyl chloride are extracted in the retort.Open stirring, heating in water bath, temperature is controlled at 80 ± 5 ℃.Reacted 72 hours; Standing demix is extracted supernatant liquid out, and lower floor's product underpressure distillation 24 hours obtains colourless viscous liquid, becomes white solid after the cooling.
Embodiment 2
1-butyl-3-Methylimidazole villaumite
75kgN-Methylimidazole and 120kg n-propylcarbinyl chloride are extracted in the retort.Open stirring, heating in water bath, temperature is controlled at 80 ± 5 ℃.Reacted 72 hours; Standing demix is extracted supernatant liquid out, and lower floor's product underpressure distillation 24 hours obtains colourless viscous liquid, becomes white solid after the cooling.
Embodiment 3
1-butyl-3-methyl imidazolium tetrafluoroborate
1-butyl-3-Methylimidazole villaumite and 55kgNaBF that 80kg is made by embodiment 1
4, being dissolved in water, the suction retort adds the 50kg methylene dichloride, stirs, normal-temperature reaction 24 hours, standing demix, after lower floor's liquid is told, washing, methylene dichloride is reclaimed in first air distillation, and underpressure distillation is 24 hours again, gets colourless viscous liquid.
Embodiment 4
1-butyl-3-Methylimidazole hexafluorophosphate
1-butyl-3-Methylimidazole villaumite and 70kgKPF that 60kg is made by embodiment 1
6Be dissolved in water, the suction retort stirs, normal-temperature reaction 24 hours, and standing demix, after lower floor's liquid is told, washing, underpressure distillation 24 hours gets colourless viscous liquid.
Embodiment 5
1-hexyl-3-methyl imidazolium tetrafluoroborate
80kg1-hexyl-3 Methylimidazole villaumite and 50kgNaBF that embodiment 1 technology is made
4, being dissolved in water, the suction retort adds the 50kg methylene dichloride, stirs, normal-temperature reaction 24 hours, standing demix, after lower floor's liquid is told, washing, methylene dichloride is reclaimed in first air distillation, and underpressure distillation is 24 hours again, gets colourless viscous liquid.
Embodiment 6
1-hexyl-3-Methylimidazole hexafluorophosphate
60kg1-hexyl-3 Methylimidazole villaumite and 60kgKPF that embodiment 1 technology is made
6, being dissolved in water, the suction retort adds the 40kg methylene dichloride, stirs, normal-temperature reaction 24 hours, standing demix, after lower floor's liquid is told, washing, methylene dichloride is reclaimed in first air distillation, and underpressure distillation is 24 hours again, gets colourless viscous liquid.
Embodiment 7
1-decyl-3-Methylimidazole hexafluorophosphate
40kg1-decyl-3 Methylimidazole bromine salt and 25kgKPF that embodiment 1 technology is made
6, being dissolved in water, the suction retort adds the 25kg methylene dichloride, stirs, normal-temperature reaction 24 hours, standing demix, after lower floor's liquid is told, washing, methylene dichloride is reclaimed in first air distillation, and underpressure distillation is 24 hours again, gets colourless viscous liquid.
Embodiment 8
1-decyl-3-Methylimidazole hexafluorophosphate
80kg1-decyl-3 Methylimidazole bromine salt and 50kgKPF that embodiment 1 technology is made
6, being dissolved in water, the suction retort adds the 50kg methylene dichloride, stirs, normal-temperature reaction 24 hours, standing demix, after lower floor's liquid is told, washing, methylene dichloride is reclaimed in first air distillation, and underpressure distillation is 24 hours again, gets colourless viscous liquid.
After the embodiment that describes in detail, being familiar with this technology personage can be well understood to, do not breaking away under above-mentioned claim and the spirit, can carry out various variations and modification, all foundations technical spirit of the present invention all belongs to the scope of technical solution of the present invention to any simple modification, equivalent variations and modification that above embodiment did.And the embodiment that the present invention also is not subject in the specification sheets to be given an actual example.
Claims (4)
1, a kind of imidazole ionic liquid production technology, such ion liquid general structure is
In the formula: R1 is the saturated hydrocarbyl that contains 1～20 carbon atom;
X
-For inorganic or organic ion unit, comprising: Cl
-, Br
-, BF
4 -, PF
6 -, CH
3COO
-, CF
3COO
-
Its production process is:
1) N-Methylimidazole and halon were extracted in the retort by the mole proportioning in 1: 1～1: 1.9, stir, heating in water bath, temperature is controlled at 20～95 ℃, reacts 24～96 hours, obtains the halogen ionic liquid; Further add respective anionic salt, stir, heating in water bath, temperature is controlled at 20～95 ℃, reacts 24～96 hours, can get corresponding ionic liquid.
2) with the reactant standing demix, the washing purifying, underpressure distillation obtains product.
2, a kind of imidazole ionic liquid production technology according to claim 1 is characterized in that: all reactants and solvent are liquid state or solution form, adopt vacuum to take out material.
3, a kind of imidazole ionic liquid production technology according to claim 1 is characterized in that: adopt methylene dichloride to make solvent for water soluble ion liquid.
4, a kind of imidazole ionic liquid production technology according to claim 3 is characterized in that: the methylene dichloride in the reaction process is recycled by underpressure distillation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910065927A CN101654438A (en) | 2009-08-14 | 2009-08-14 | Imidazole ionic liquid production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910065927A CN101654438A (en) | 2009-08-14 | 2009-08-14 | Imidazole ionic liquid production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101654438A true CN101654438A (en) | 2010-02-24 |
Family
ID=41708921
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910065927A Pending CN101654438A (en) | 2009-08-14 | 2009-08-14 | Imidazole ionic liquid production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101654438A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167683A (en) * | 2011-02-23 | 2011-08-31 | 中国科学院过程工程研究所 | Bivalent cation magnetic ionic liquids and preparation method thereof |
| CN102229567A (en) * | 2011-04-28 | 2011-11-02 | 广东工业大学 | Method for purifying 1-alkyl-3-methylimidazole tetrafluoro borate ionic liquid |
| CN102351796A (en) * | 2011-08-23 | 2012-02-15 | 林州市科能材料科技有限公司 | Production process of imidazole ionic liquid |
| CN105130902A (en) * | 2015-09-05 | 2015-12-09 | 侯颖 | Preparation method of ionic liquid |
| CN106543084A (en) * | 2016-09-28 | 2017-03-29 | 山东源根石油化工有限公司 | A kind of preparation of 3 Methylimidazole. hexafluorophosphoric acid ionic liquid of 1 hexyl and the fire resistant hydraulic fluid containing the ionic liquid |
| CN107501185A (en) * | 2016-06-14 | 2017-12-22 | 赢创德固赛有限公司 | The method for purifying ionic liquid |
| CN107641104A (en) * | 2017-11-24 | 2018-01-30 | 林州市科能材料科技有限公司 | The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 |
| CN114591181A (en) * | 2022-03-24 | 2022-06-07 | 宁波原力新材料有限公司 | Method for preparing high-purity ionic liquid |
-
2009
- 2009-08-14 CN CN200910065927A patent/CN101654438A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167683A (en) * | 2011-02-23 | 2011-08-31 | 中国科学院过程工程研究所 | Bivalent cation magnetic ionic liquids and preparation method thereof |
| CN102229567A (en) * | 2011-04-28 | 2011-11-02 | 广东工业大学 | Method for purifying 1-alkyl-3-methylimidazole tetrafluoro borate ionic liquid |
| CN102351796A (en) * | 2011-08-23 | 2012-02-15 | 林州市科能材料科技有限公司 | Production process of imidazole ionic liquid |
| CN105130902A (en) * | 2015-09-05 | 2015-12-09 | 侯颖 | Preparation method of ionic liquid |
| CN107501185A (en) * | 2016-06-14 | 2017-12-22 | 赢创德固赛有限公司 | The method for purifying ionic liquid |
| CN107501185B (en) * | 2016-06-14 | 2022-08-16 | 赢创运营有限公司 | Method for purifying ionic liquids |
| CN106543084A (en) * | 2016-09-28 | 2017-03-29 | 山东源根石油化工有限公司 | A kind of preparation of 3 Methylimidazole. hexafluorophosphoric acid ionic liquid of 1 hexyl and the fire resistant hydraulic fluid containing the ionic liquid |
| CN106543084B (en) * | 2016-09-28 | 2019-04-12 | 山东源根石油化工有限公司 | A kind of preparation of 1- hexyl -3- methylimidazole hexafluorophosphoric acid ionic liquid and fire resistant hydraulic fluid containing the ionic liquid |
| CN107641104A (en) * | 2017-11-24 | 2018-01-30 | 林州市科能材料科技有限公司 | The preparation method of the methylimidazole villaumite ionic liquid of 1 ethyl 3 |
| CN114591181A (en) * | 2022-03-24 | 2022-06-07 | 宁波原力新材料有限公司 | Method for preparing high-purity ionic liquid |
| CN114591181B (en) * | 2022-03-24 | 2024-04-19 | 原力新材料(合肥)有限公司 | Method for preparing high-purity ionic liquid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101654438A (en) | Imidazole ionic liquid production technology | |
| CN101386597B (en) | Alkyl imidazoles perrhenate ion liquid and preparation method thereof | |
| CN101092399A (en) | Method for preparing ionic liquid with anion being as ion in halogen family | |
| CN100532365C (en) | Method of continuously synthesizing ionic liquid at room temperature | |
| CN102050788B (en) | Method for synthesizing halogen-free imidazole ionic liquid | |
| CN101633641B (en) | Preparation method of imidazole type ionic liquid | |
| JP5075870B2 (en) | Method for producing quaternary ammonium tetrafluoroborate | |
| CN101941986A (en) | Y aromatic ligand ionic liquid and preparation method thereof | |
| CN103613672A (en) | Method for preparing cellulose acetate by employing ionic liquid as catalyst | |
| CN101659611B (en) | Method for preparing 2, 4, 5-trifluoro-phenylacetic-acid | |
| CN103694113A (en) | Method for preparing paraphthaloyl chloride | |
| KR20100042264A (en) | Method for production of purified ammonium salt of fluorinated bis-sulfonylimide | |
| CN104829813B (en) | A kind of ionomeric polymer containing phosphine, preparation method and anion-exchange membrane | |
| CN113481524A (en) | Preparation method for electrochemically synthesizing 3-trifluoromethyl coumarin compound | |
| CN102351796A (en) | Production process of imidazole ionic liquid | |
| CN113277982A (en) | Method and reaction device for continuously preparing 2-trifluoromethyl-4, 5-dicyanoimidazole lithium salt | |
| CN102020610A (en) | Low-viscosity ionic liquid | |
| CN102977031A (en) | Method for synthesizing ionic liquid | |
| CN100532359C (en) | Method of synthesizing ion liquid at room temperature | |
| CN102766075A (en) | Double-acid-level contained quaternary ammonium salt ionic liquid and preparation method thereof | |
| CN101781250A (en) | Method for synthesizing low bromine content iminazole ionic liquid | |
| CN107759637A (en) | The fluoridation catalyst of a kind of phosphonitrile and phosphazene derivative and its synthetic method of fluoride | |
| CN114591181A (en) | Method for preparing high-purity ionic liquid | |
| CN103787847B (en) | A kind of take ionic liquid as the technique of solvent continuous production trimethyl orthoacetate | |
| CN113957461A (en) | Electrochemical synthesis method of 1,1' -binaphthyl compound |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100224 |